CN112694080A - Carbon microsphere with embedded conductive network structure, preparation method and energy storage application thereof - Google Patents

Carbon microsphere with embedded conductive network structure, preparation method and energy storage application thereof Download PDF

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CN112694080A
CN112694080A CN202011606935.6A CN202011606935A CN112694080A CN 112694080 A CN112694080 A CN 112694080A CN 202011606935 A CN202011606935 A CN 202011606935A CN 112694080 A CN112694080 A CN 112694080A
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carbon
network structure
olive oil
conductive network
mixed solution
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CN112694080B (en
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宋怀河
袁满
刘海燕
陈晓红
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Beijing University of Chemical Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention provides a carbon microsphere with an embedded conductive network structure, a preparation method and an energy storage application thereof, and relates to the field of electrode materials of lithium ion batteries and sodium ion batteries. The particle size of the material is 1-20 microns, and the nano conductive material is uniformly distributed in the sphere and forms a three-dimensional network structure with matrix carbon. Mixing glucose or sucrose with a high-conductivity material to prepare a uniform mixed solution; then spraying it into the high-temperature oliveCooling to room temperature, separating the globules from the olive oil, and washing; and putting the product into a high-temperature carbonization furnace, and heating to 800-1400 ℃ in a nitrogen atmosphere to obtain the final product. The specific surface area of the prepared carbon microsphere is 100m2g‑1Below, the tap density was 0.7g ml‑1The above. When the material is used as a negative electrode material of a lithium ion battery and a sodium ion battery, the material shows high reversible capacity and cycling stability, and particularly high-rate charge and discharge performance.

Description

Carbon microsphere with embedded conductive network structure, preparation method and energy storage application thereof
Technical Field
The invention relates to the field of lithium ion battery electrode materials, in particular to a carbon microsphere with an embedded conductive network structure, a preparation method and an energy storage application thereof.
Background
The lithium ion battery has the advantages of good cycle stability, small self-discharge, high specific energy and the like, and is widely applied to the field of energy storage. With the rapid development of the field of electric automobiles, people put higher requirements on the energy density and the power density of lithium ion batteries. Meanwhile, the characteristics of limited lithium resource reserves, uneven distribution and the like also limit the further development of the lithium ion battery. Sodium has electrochemical properties similar to those of lithium and is abundant in reserves, so that the sodium-ion battery is expected to be a supplement and a substitute for a lithium-ion battery.
The main factor limiting the improvement of the performance of lithium/sodium ion batteries is that the electrode material, especially the negative electrode material, is crucial to the development of lithium/sodium ion batteries. At present, the cathode materials widely used for lithium ion batteries are mainly graphite materials, but the capacity of the materials is improved by the theoretical capacity of 372mA h/g. Researches find that the hard carbon microsphere material shows excellent lithium and sodium storage performance by virtue of the unique morphological structure characteristics of the hard carbon microsphere material. First, the large carbon interlayer topology, rich microporous structure and defect sites exhibited by hard carbon-based materials all contribute to the storage of lithium/sodium ions, thereby increasing the energy density of the material. On the other hand, the regular spherical structure enables the cathode material to have the characteristics of high tap density, stable structure, isotropy and the like, and is beneficial to improving the volume specific capacity and the cycling stability of the cathode material. However, the arrangement of the graphite micro-domains intermittently dislocated in the hard carbon material can affect the transmission and diffusion of ions and electrons, and finally affect the rate capability of the material. The hard carbon microsphere material is structurally modified, the rate capability of the hard carbon microsphere material is improved, and the hard carbon microsphere material becomes the focus of the research on the cathode of the lithium/sodium ion battery at present.
The composite material is compounded with a hard carbon material by adding high-conductivity materials such as graphene, carbon nanotubes, Mxene and the like, so that the composite material is an effective means for improving the rate capability of the composite material. In patent CN102544459B, "method for preparing graphene coated carbon microsphere material by coating graphene oxide on carbon microsphere", graphene oxide is coated on the surface of carbon microsphere, and a conductive network is constructed between carbon microspheres, so as to improve the conductive performance of the material as a negative electrode of a lithium ion battery. An article entitled "Hard CARBON microspheres interconnected by CARBON nanotubes as high-performance and materials for sodium-ion batteries" published by Liyao Suo et al in CARBON (151,2019,1-9) connects CARBON microspheres through CARBON nanotubes to prepare a grape-shaped structure, and also improves the diffusion rate of electrons and sodium ions between the CARBON microspheres by introducing the CARBON nanotubes with high conductivity, thereby improving the rate capability of the sodium-ion battery.
The modification methods reported above all have some problems in the practical application process. First, these composite modification methods are limited to the surface of the carbon microspheres, and do not improve the electron/ion diffusion process inside the carbon microspheres. Secondly, materials such as graphene and carbon nanotubes generally have the characteristics of high specific surface area, low density and the like, and the overall density of the material can be reduced after the materials are compounded with carbon microspheres, so that the volume specific capacity of the material is influenced. Third, the added highly conductive material generally has higher reactivity, and when directly exposed to the electrolyte, more electrolyte is consumed in the previous charging and discharging processes, resulting in higher irreversible capacity and lower coulombic efficiency.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a carbon microsphere with an embedded conductive network structure, a preparation method and an energy storage application thereof, and the carbon microsphere is characterized in that:
the diameter of the carbon microsphere obtained by the invention is between 1 and 20 micrometers, and the specific surface area is between 50 and 100m2The tap density is between 0.7 and 1.2g/ml, the added high-conductivity material is uniformly embedded and dispersed in the sphere to form a uniform embedded conductive network, and the surface and the inside of the microsphere both present a fold structure.
The preparation method of the carbon microsphere comprises the following steps:
step 1): mixing a certain amount of high-conductivity material with glucose or sucrose as a carbon source, dispersing the mixture into deionized water, and performing ultrasonic treatment, stirring and other treatment to form a uniform mixed solution;
step 2): measuring a certain amount of olive oil, heating the system to 100-150 ℃ at a certain stirring rate, and then spraying the mixed solution prepared in the step 1) into the olive oil; after the solution is sprayed, cooling to room temperature, separating the globules from the olive oil, washing and drying;
step 3): and (3) putting the product into a high-temperature carbonization furnace, and heating to 800-1400 ℃ in a nitrogen atmosphere to obtain a final product.
The carbon source is selected from glucose or sucrose, and the high-conductivity material is selected from one or more of one-dimensional or two-dimensional materials such as carbon nanotubes, graphene oxide, Mxene and the like.
The mass of the high-conductivity material accounts for 0.1-10% of the mass of the glucose or the sucrose. The concentration of sucrose or glucose in the mixed solution is 1-50 mg ml-1。
The volume ratio of the sprayed mixed solution to the olive oil in the step 2) is 1/10-1/1.
The invention obtains the carbon microsphere with the embedded conductive network structure, and the carbon microsphere is applied to the negative electrode material of lithium and sodium ion batteries.
Compared with the prior art, the invention has the advantage that the high-conductivity material is embedded in the carbon microspheres. This embedded structure can effectively improve the electronic/ionic conductivity inside the particles, not just change the conductivity between particles. The same amount of addition can give a better modification effect than in the case of the outer coating or the connecting structure only. In the embedded structure, the highly conductive material dispersed in the carbon microspheres and the carbon matrix are connected with each other by chemical bonds, so that the material becomes more compact, and the volume ratio capacity is favorably improved. In addition, the embedded structure also avoids direct contact of the high-reactivity materials and the electrolyte, and is beneficial to maintaining higher coulombic efficiency and cycling stability.
Drawings
FIG. 1 is a scanning electron microscope image of a carbon microsphere with an embedded conductive network structure according to example 1 of the present invention;
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, but the present invention is not limited to the following examples. The following examples are conditions for electrode testing when used as a lithium ion battery negative electrode material: the electrode composition is 80% of the carbon microsphere, 10% of acetylene black and 10% of PVDF, and the electrolyte composition is 1mol of LiPF6Dissolved in a solvent with a volume ratio of EC to DEC of 1: 1. Conditions of electrode test when used as a negative electrode material of a sodium ion battery: the electrode composition is 80% of the carbon microsphere, 10% of acetylene black and 10% of PVDF, and the electrolyte composition is 1mol of NaPF6Dissolved in a solvent with a volume ratio of EC to DEC of 1: 1.
Example 1
Taking 5g of glucose and 50mg of graphene, wherein the thickness is about 2nm, adding the glucose and the graphene into 100ml of deionized water, and carrying out ultrasonic treatment, stirring and other treatment to form a uniform mixed solution; measuring 200ml of olive oil, heating the system to 120 ℃ at a stirring speed of 100r/min, and then spraying the prepared mixed solution into the olive oil; after the solution is sprayed, cooling to room temperature, separating the globules from the olive oil, and washing with ethanol; and putting the product into a high-temperature carbonization furnace, and heating to 800 ℃ in a nitrogen atmosphere to obtain a final product. The specific surface area is 89m2g-1Tap density of 0.85g ml-1。
The interior of the carbon microsphere shows a graphene embedded structure as shown in a Scanning Electron Microscope (SEM) of figure 1.
The electrochemical performance test result shows that when the electrode material is used as the negative electrode material of the lithium ion battery, the amount of the electrode material is 0.05mA g-1The specific discharge capacity under the current density can reach 465mA h g-1(ii) a At 10A g-1The discharging specific capacity can still be maintained at 142mA h g under the current density-1. When the material is used as a negative electrode material of a sodium ion battery, the concentration is 0.05mA g-1The specific discharge capacity under the current density can reach 302mA h g-1(ii) a At 10A g-1Current density lowering ofThe specific capacity can still be kept at 95mA h g-1。
Example 2
5g of sucrose and 100mg of carbon nanotubes are taken, the diameter of the carbon tube is 3.2nm, and the length of the carbon tube is 1.8 mu m. Adding into 200ml deionized water, and performing ultrasonic treatment, stirring and the like to form a uniform mixed solution; measuring 200ml of olive oil, heating the system to 130 ℃ at a stirring speed of 100r/min, and then spraying the prepared mixed solution into the olive oil; after the solution is sprayed, cooling to room temperature, separating the globules from the olive oil, and washing with ethanol; and putting the product into a high-temperature carbonization furnace, and heating to 1200 ℃ in a nitrogen atmosphere to obtain a final product. The specific surface area is 78m2g-1Tap density of 0.91g ml-1。
The electrochemical performance test result shows that when the electrode material is used as the negative electrode material of the lithium ion battery, the amount of the electrode material is 0.05mA g-1The specific discharge capacity under the current density can reach 408mA h g-1(ii) a At 10A g-1The discharging specific capacity can still be maintained at 123mA h g under the current density-1. When the material is used as a negative electrode material of a sodium ion battery, the concentration is 0.05mA g-1The specific discharge capacity under the current density can reach 286mA h g-1(ii) a At 10A g-1The discharge specific capacity can still be kept at 89mA h g under the current density-1。
Example 3
5g of glucose and 200mg of Mxene were taken and the thickness was 2.4 nm. Adding into 300ml deionized water, and forming uniform mixed solution after ultrasonic treatment, stirring and the like; measuring 200ml of olive oil, heating the system to 130 ℃ at a stirring speed of 100r/min, and then spraying the prepared mixed solution into the olive oil; after the solution is sprayed, cooling to room temperature, separating the globules from the olive oil, and washing with ethanol; and putting the product into a high-temperature carbonization furnace, and heating to 800 ℃ in a nitrogen atmosphere to obtain a final product. Specific surface area of 92m2g-1Tap density of 0.84g ml-1。
The electrochemical performance test result shows that the electrode material is used as the negative electrode material of the lithium ion batteryWhen the material is used, the ratio is 0.05mAg-1The discharge specific capacity under the current density can reach 396mA h g-1(ii) a At 10A g-1The discharging specific capacity can still be kept at 145mA h g under the current density-1. When the material is used as a negative electrode material of a sodium ion battery, the concentration is 0.05mA g-1The specific discharge capacity under the current density can reach 291mA h g-1(ii) a At 10A g-1The discharging specific capacity can still be kept at 103mA h g under the current density-1。
Example 4
Adding 5g of sucrose, 100mg of graphene (about 2nm in thickness) and 200mg of Mxene (about 2.4nm in thickness) into 500ml of deionized water, and performing ultrasonic treatment, stirring and the like to form a uniform mixed solution; measuring 200ml of olive oil, heating the system to 140 ℃ at a stirring speed of 100r/min, and then spraying the prepared mixed solution into the olive oil; after the solution is sprayed, cooling to room temperature, separating the globules from the olive oil, and washing with ethanol; and putting the product into a high-temperature carbonization furnace, and heating to 800 ℃ in a nitrogen atmosphere to obtain a final product. Specific surface area of 91m2g-1Tap density of 0.79g ml-1。
The electrochemical performance test result shows that when the electrode material is used as the negative electrode material of the lithium ion battery, the amount of the electrode material is 0.05mA g-1The specific discharge capacity under the current density can reach 419mA h g-1(ii) a At 10A g-1The discharging specific capacity can still be kept at 151mA h g under the current density-1. When the material is used as a negative electrode material of a sodium ion battery, the concentration is 0.05mA g-1The specific discharge capacity under the current density can reach 311mA h g-1(ii) a At 10A g-1The discharging specific capacity can still be maintained at 109mA h g under the current density-1。
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (6)

1. A carbon microsphere with an embedded conductive network structure, a preparation method and an energy storage application thereof are characterized in that: the diameter of the sphere is between 1 and 20 microns, and the specific surface area is between 50 and 100m2The tap density is between 0.7 and 1.2g/ml, the added high-conductivity material is uniformly embedded and dispersed in the sphere to form a uniform embedded conductive network, and the surface and the inside of the microsphere both present a fold structure.
2. The carbon microsphere with the embedded conductive network structure, the preparation method and the energy storage application thereof as claimed in claim 1 are characterized in that the carbon microsphere is prepared by the following method:
step 1): mixing a certain amount of high-conductivity material with glucose or sucrose as a carbon source, dispersing the mixture into deionized water, and performing ultrasonic treatment, stirring and other treatment to form a uniform mixed solution;
step 2): measuring a certain amount of olive oil, heating the system to 100-150 ℃ at a certain stirring rate, and then spraying the mixed solution prepared in the step 1) into the olive oil; after the solution is sprayed, cooling to room temperature, separating the globules from the olive oil, washing and drying;
step 3): and (3) putting the product into a high-temperature carbonization furnace, and heating to 800-1400 ℃ in a nitrogen atmosphere to obtain a final product.
3. The method of claim 2, wherein: the carbon source is selected from glucose or sucrose, and the high-conductivity material is selected from one or more of one-dimensional or two-dimensional materials such as carbon nanotubes, graphene oxide, Mxene and the like.
4. The method of claim 2, wherein: the mass of the high-conductivity material accounts for 0.1-10% of the mass of the glucose or the sucrose. The concentration of sucrose or glucose in the mixed solution is 1-50 mg ml-1。
5. The method of claim 2, wherein: the volume ratio of the mixed solution to the olive oil is 1/10-1/1.
6. Use of the carbon microspheres with embedded conductive network structure obtained by the method of claims 1 to 5 as negative electrode materials of lithium/sodium ion batteries.
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CN113909072A (en) * 2021-08-27 2022-01-11 青岛科技大学 Preparation method of metal-doped porous carbon microsphere/CNTs composite material
CN114430030A (en) * 2022-01-14 2022-05-03 北京化工大学 Soft carbon with multi-interface structure, preparation method and energy storage application thereof
CN115799449A (en) * 2022-12-12 2023-03-14 双登集团股份有限公司 Sodium ion battery and manufacturing process thereof

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CN115799449A (en) * 2022-12-12 2023-03-14 双登集团股份有限公司 Sodium ion battery and manufacturing process thereof

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